Comprehensive solid-state characterization of rare earth fluoride nanoparticles

Lucier, B.E.G. and Johnston, K.E. and Arnold, Donna C. and Lemyre, J.-L. and Beaupré, A. and Blanchette, M. and Ritcey, A.M. and Schurko, R.W. (2014) Comprehensive solid-state characterization of rare earth fluoride nanoparticles. Journal of Physical Chemistry C, 118 (2). pp. 1213-1228. ISSN 1932 7447. (doi:https://doi.org/10.1021/jp408148b) (The full text of this publication is not currently available from this repository. You may be able to access a copy if URLs are provided)

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Official URL
http://dx.doi.org/10.1021/jp408148b

Abstract

The combination of multinuclear solid-state NMR spectroscopy and powder X-ray diffraction has been applied to characterize the octahedron-shaped crystalline nanoparticle products resulting from an inverse micelle synthesis. Rietveld refinements of the powder X-ray diffraction data from the nanoparticles revealed their general formula to be (H3O)Y3F 10·xH2O. 1H magic-angle spinning (MAS) NMR experiments provided information on sample purity and served as an excellent probe of the zeolithic incorporation of atmospheric water. 19F MAS NMR experiments on a series of monodisperse nanoparticle samples of various sizes yielded spectra featuring three unique 19F resonances arising from three different fluorine sites within the (H3O)Y 3F10·xH2O crystal structure. Partial removal of zeolithic water from the internal cavities and tunnels of the nanoparticles led to changes in the integrated peak intensities in the 19F MAS NMR spectra; the origin of this behavior is discussed in terms of 19F longitudinal relaxation. 19F-89Y variable-amplitude cross-polarization (VACP) NMR experiments on both stationary samples and samples under MAS conditions indicated that two distinct yttrium environments are present, and on the basis of the relative peak intensities, the population of one of the two sites is closely linked to the nanoparticle size. Both 19F MAS and 19F-89Y VACP/MAS experiments indicated small amounts of an impurity present in certain nanoparticles; these are postulated to be spherical amorphous YF3 nanoparticles. We discuss the importance of probing molecular-level structure in addition to microscopic structure and how the combination of these characterization methods is crucial for understanding nanoparticle design, synthesis, and application. © 2013 American Chemical Society.

Item Type: Article
Additional information: Unmapped bibliographic data: LA - English [Field not mapped to EPrints] J2 - J. Phys. Chem. C [Field not mapped to EPrints] AD - Department of Chemistry and Biochemistry, University of Windsor, Windsor, ON N9B 3P4, Canada [Field not mapped to EPrints] AD - School of Physical Sciences, University of Kent, Canterbury, Kent CT2 7NH, United Kingdom [Field not mapped to EPrints] AD - Department of Chemistry and CERMA, Université Laval, Québec, G1V 0A6, Canada [Field not mapped to EPrints] DB - Scopus [Field not mapped to EPrints]
Uncontrolled keywords: Characterization methods, Crystalline nanoparticles, Longitudinal relaxation, Monodisperse nanoparticles, Powder X ray diffraction, Rare earth fluoride nanoparticles, Relative peak intensity, Solid-state NMR spectroscopy, Magic angle spinning, Nanoparticles, Nuclear magnetic resonance spectroscopy, Rietveld refinement, X ray diffraction, Synthesis (chemical)
Subjects: Q Science > QC Physics > QC176.8.N35 Nanoscience, nanotechnology
Divisions: Faculties > Sciences > School of Physical Sciences
Faculties > Sciences > School of Physical Sciences > Functional Materials Group
Depositing User: Giles Tarver
Date Deposited: 07 Jul 2015 10:48 UTC
Last Modified: 14 Feb 2019 15:11 UTC
Resource URI: https://kar.kent.ac.uk/id/eprint/49057 (The current URI for this page, for reference purposes)
Arnold, Donna C.: https://orcid.org/0000-0003-0239-5790
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